US11851370B2 - Laminated body for preparing wavelength conversion member and preparation method of wavelength conversion member - Google Patents

Laminated body for preparing wavelength conversion member and preparation method of wavelength conversion member Download PDF

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Publication number
US11851370B2
US11851370B2 US16/562,635 US201916562635A US11851370B2 US 11851370 B2 US11851370 B2 US 11851370B2 US 201916562635 A US201916562635 A US 201916562635A US 11851370 B2 US11851370 B2 US 11851370B2
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green sheet
wavelength converting
converting member
mole
confining layer
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US20200079684A1 (en
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Min Suk Kang
Jung Kyu Lee
Seung Jae Lee
Joong Kyu LIM
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Dae Joo Electronic Materials Co Ltd
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Dae Joo Electronic Materials Co Ltd
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Assigned to DAEJOO ELECTRONIC MATERIALS CO., LTD. reassignment DAEJOO ELECTRONIC MATERIALS CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KANG, MIN SUK, LEE, JUNG KYU, LEE, SEUNG JAE, LIM, JOONG KYU
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00—Compositions for glass with special properties
    • C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/85—Packages
    • H10H20/851—Wavelength conversion means
    • H10H20/8511—Wavelength conversion means characterised by their material, e.g. binder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/068—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/16—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating
    • B32B37/18—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating involving the assembly of discrete sheets or panels only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/16—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer formed of particles, e.g. chips, powder or granules
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C12/00—Powdered glass; Bead compositions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/006—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of microcrystallites, e.g. of optically or electrically active material
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/08—Frit compositions, i.e. in a powdered or comminuted form containing phosphorus
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7706—Aluminates
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/01—Manufacture or treatment
    • H10H20/036—Manufacture or treatment of packages
    • H10H20/0361—Manufacture or treatment of packages of wavelength conversion means
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/85—Packages
    • H10H20/851—Wavelength conversion means
    • H10H20/8514—Wavelength conversion means characterised by their shape, e.g. plate or foil
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
    • B32B2264/10—Inorganic particles
    • B32B2264/102—Oxide or hydroxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/422—Luminescent, fluorescent, phosphorescent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/732—Dimensional properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2315/00—Other materials containing non-metallic inorganic compounds not provided for in groups B32B2311/00 - B32B2313/04
    • B32B2315/08—Glass
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2551/00—Optical elements
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2204/00—Glasses, glazes or enamels with special properties
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2214/00—Nature of the non-vitreous component
    • C03C2214/04—Particles; Flakes

Definitions

  • the present invention relates to a laminate for preparing a wavelength converting member and a process for preparing a wavelength converting member. More particularly, the present invention relates to a laminate for preparing a wavelength converting member having a high total light transmittance and excellent optical characteristics, and a process for efficiently preparing the wavelength converting member using a confining layer comprised of specific components.
  • LEDs Light emitting diodes used for conventional lighting and the like are generally composed of blue LEDs and wavelength converting members that absorb blue light emitted from the blue LEDs and achieve white light through the emission of yellow, green, or red light.
  • the wavelength converting member may be prepared by preparing a green sheet for forming a wavelength converting member that generally comprises glass, followed by laminating a confining layer for controlling the shape of the green sheet on one side or both sides of the green sheet and calcining the laminate. However, if the confining layer is laminated on only one side of the green sheet and calcined, the green sheet may be shrunk unevenly during the calcination, thereby impairing the shape of the wavelength converting member thus prepared.
  • Korean Patent No. 10-0930165 discloses a process of disposing a first confining layer that comprises an alumina powder on both sides of a green sheet that comprises a glass component and disposing a second confining layer that comprises a combustible material on each of the exposed sides of the first confining layer, thereby preparing a multilayered ceramic substrate.
  • the green sheet melt i.e., a glass melt, which has a low viscosity at a high temperature during calcination after the lamination, penetrates between the alumina particles used as a component of the first confining layer to form a thin layer on the interface between the two layers.
  • the confining layers are removed by polishing and/or etching after the calcination, the layer formed between the green sheet and the confining layer is not completely removed but remains on the surface of the wavelength converting member, thereby reflecting light emitted from a light source.
  • it has a disadvantage that the amount of light to reach a phosphor is reduced.
  • An object of the present invention is to provide a laminate for preparing a wavelength converting member, which is capable of being calcined at a temperature of 800° C. or lower, preferably 700° C. or lower and having a high light transmittance, a high refractive index, and a good shape upon the calcination, and a process for efficiently preparing the wavelength converting member.
  • the present invention provides a laminate for preparing a wavelength converting member, which comprises a green sheet for forming the wavelength converting member, which comprises a glass matrix and an inorganic phosphor powder dispersed in the glass matrix; a green sheet for a confining layer A, which comprises a silica powder only as an inorganic oxide powder and is disposed on both sides of the green sheet for forming the wavelength converting member; and a green sheet for a confining layer B disposed on both sides of the green sheet for the confining layer A, which are not in contact with the green sheet for forming the wavelength converting member, wherein the glass matrix comprises 0.1 to 15% by mole of P 2 O 5 , 20 to 50% by mole of ZnO, 8 to 40% by mole of SiO 2 , and 10 to 30% by mole of B 2 O 3 , based on the total number of moles of the glass powder.
  • the present invention provides a process for preparing a wavelength converting member, which comprises a first step of preparing a green sheet for forming the wavelength converting member, which comprises a glass powder and an inorganic phosphor powder; a second step of disposing a green sheet for a confining layer A, which comprises a silica powder only as an inorganic oxide powder, on both sides of the green sheet for forming the wavelength converting member; a third step of disposing a green sheet for a confining layer B on both sides of the green sheet for the confining layer A, which are not in contact with the green sheet for forming the wavelength converting member, and laminating them to obtain a laminate; a fourth step of calcining the laminate; and a fifth step of removing the calcined confining layer A and confining layer B from the calcined laminate.
  • the present invention provides a wavelength converting member prepared through the above preparation process.
  • the wavelength converting member according to the present member can be prepared by the calcination at a temperature of 800° C. or lower, preferably 700 IC or lower and has a high light transmittance, a high refractive index, and a good shape upon the calcination. Thus, it can be advantageously used for LEDs.
  • the laminate for preparing a wavelength converting member of the present invention comprises a green sheet for forming the wavelength converting member, which comprises a glass matrix and an inorganic phosphor powder dispersed in the glass matrix; a green sheet for a confining layer A, which comprises a silica powder only as an inorganic oxide powder and is disposed on both sides of the green sheet for forming the wavelength converting member; and a green sheet for a confining layer B disposed on both sides of the green sheet for the confining layer A, which are not in contact with the green sheet for forming the wavelength converting member, wherein the glass matrix comprises 0.1 to 15% by mole of P 2 O 5 , 20 to 50% by mole of ZnO, 8 to 40% by mole of SiO 2 , and 10 to 30% by mole of B 2 O 3 , based on the total number of moles of the glass powder.
  • the glass matrix comprises 0.1 to 15% by mole of P 2 O 5 , 20 to 50% by mole of ZnO, 8 to 40% by mole of SiO 2 , and 10 to 30% by mole of B 2 O 3 , based on the total number of moles of the glass powder.
  • the glass matrix comprises 0.1 to 13% by mole, 0.1 to 10% by mole, or 0.2 to 10% by mole of P 2 O 5 ; 25 to 50% by mole, 25 to 48% by mole, or 28 to 48% by mole of ZnO; 8 to 38% by mole, 8 to 36% by mole, or 8 to 35% by mole of SiO 2 ; and 11 to 30% by mole, 11 to 28% by mole, or 11 to 27% by mole of B 2 O 3 , based on the total number of moles of the glass powder.
  • the glass matrix may further comprise 0.1 to 20% by mole of SnO 2 and 0.1 to 20% by mole of Al 2 O 3 , based on the total number of moles of the glass powder.
  • the glass matrix may further comprise 0.1 to 15% by mole, 0.1 to 10% by mole, 0.1 to 8% by mole, or 0.1 to 6% by mole of SnO 2 ; and 0.1 to 15% by mole, 0.5 to 15% by mole, 1 to 13% by mole, or 1 to 11% by mole of Al 2 O 3 , based on the total number of moles of the glass powder.
  • the glass matrix may further comprise at least one alkaline earth metal oxide selected from the group consisting of BaO, SrO, and CaO in an amount of 1 to 30% by mole based on the total number of moles of the glass powder.
  • the glass matrix may further comprise at least one alkaline earth metal oxide selected from the group consisting of BaO, SrO, and CaO in an amount of 1 to 20% by mole, 1 to 10% by mole, or 1 to 8% by mole, based on the total number of moles of the glass powder.
  • the glass matrix may further comprise at least one alkaline metal oxide selected from the group consisting of Na 2 O, K 2 O, and Li 2 O in an amount of 1 to 30% by mole based on the total number of moles of the glass powder.
  • the glass matrix may further comprise at least one alkaline metal oxide selected from the group consisting of Na 2 O, K 2 O, and Li 2 O in an amount of 1 to 20% by mole, 1 to 18% by mole, or 2 to 17% by mole, based on the total number of moles of the glass powder.
  • the glass matrix may comprise 1 to 10% by mole or 1.5 to 8% by mole of Na 2 O; 0 to 10% by mole, 0 to 8% by mole, or 0 to 7% by mole of K 2 O; and 0 to 10% by mole, 0 to 8% by mole, or 0 to 7% by mole of Li 2 O, based on the total number moles of the glass powder.
  • the alkaline metal oxide comprises Na 2 O and K 2 O; Na 2 O and Li 2 O; or Na 2 O, K 2 O, and Li 2 O.
  • the glass matrix may have a refractive index of 1.4 to 1.7 and may be derived from a glass powder having a softening point (Ts) of 400 to 700° C. and an average particle diameter (D 50 ) of 0.1 to 20 ⁇ m.
  • the glass matrix may have a refractive index of 1.45 to 1.7, 1.5 to 1.66, 1.55 to 1.65, or 1.58 to 1.66, and may be derived from a glass powder having a softening point (Ts) of 400 to 700° C., 500 to 700° C., 550 to 700° C., or 550 to 650° C., and an average particle diameter (D 50 ) of 0.1 to 20 ⁇ m, 1 to 20 ⁇ m, or 1 to 10 ⁇ m.
  • the inorganic phosphor powder may comprise at least one phosphor powder selected from the group consisting of yttrium-aluminum-garnet (YAG)-based, ruthenium-aluminum-garnet (LuAG)-based, nitride-based, sulfide-based, and silicate-based materials.
  • YAG yttrium-aluminum-garnet
  • LuAG ruthenium-aluminum-garnet
  • nitride-based nitride-based
  • sulfide-based silicate-based materials.
  • the inorganic phosphor powder may have an average particle diameter (D 50 ) of 1 to 50 ⁇ m. Specifically, the inorganic phosphor powder may have an average particle diameter (D 50 ) of 1 to 50 ⁇ m, 5 to 40 ⁇ m, or 10 to 30 ⁇ m.
  • the green sheet for forming a wavelength converting member comprises a glass matrix and an inorganic phosphor powder dispersed in the glass matrix.
  • the green sheet for forming a wavelength converting member may be prepared from a glass composition that comprises a glass powder, an inorganic phosphor powder, a binder resin, and a solvent.
  • the glass composition may comprise 3 to 160 parts by weight of an inorganic phosphor powder and 120 to 280 parts by weight of a glass powder per 100 parts by weight of a binder resin.
  • the solvent may be contained in an amount suitable for the characteristics and drying conditions of the composition. Specifically, the solvent may be contained in an amount of 30 to 50% by weight based on the total weight of the glass composition.
  • the solvent may have a low boiling point for the rapid preparation of the green sheet. Specifically, the solvent may have a boiling point of 30 to 150° C. More specifically, the solvent may have a boiling point of 60 to 130° C.
  • the solvent may comprise at least one selected from the group consisting of toluene, ethanol, butanol, acetone, and methanol.
  • the solvent may comprise at least one selected from the group consisting of toluene, ethanol, and butanol. More specifically, the solvent may comprise toluene, ethanol, and butanol.
  • the binder resin may comprise at least one selected from the group consisting of polyvinyl butyral (PVB), polyvinyl alcohol (PVA), and poly(vinyl acetate) (PVAc).
  • the binder resin may comprise polyvinyl butyral (PVB) or polyvinyl alcohol (PVA).
  • the binder resin may have a weight average molecular weight of 1,000 to 70,000 g/mole. Specifically, the binder resin may have a weight average molecular weight of 20,000 to 60,000 g/mole.
  • the glass composition may further comprise a plasticizer.
  • the plasticizer may comprise at least one selected from the group consisting of DOP (dioctyl phthalate), DOA (dioctyl adipate), and TCP (tricresyl phosphate).
  • the plasticizer may comprise DOP (dioctyl phthalate) or DOA (dioctyl adipate).
  • the plasticizer may be contained in an amount of 10 to 200 parts by weight per 100 parts by weight of the binder resin. Specifically, the plasticizer may be contained in an amount of 30 to 90 parts by weight per 100 parts by weight of the binder resin.
  • the glass composition may be prepared by mixing a solvent and a binder resin, removing bubbles, and then adding thereto a glass powder, an inorganic phosphor powder, a plasticizer, and the like. Since a solvent having a low boiling point is used in the present invention, the binder resin and the solvent can be mixed at room temperature in the preparation of the glass composition.
  • the green sheet for forming a wavelength converting member may comprise 30 to 100% by weight of a glass matrix and 5 to 50% by weight of an inorganic phosphor powder based on the total weight of the green sheet.
  • the green sheet for forming a wavelength converting member may comprise 40 to 90% by weight of a glass matrix and 8 to 30% by weight of an inorganic phosphor powder based on the total weight of the green sheet.
  • the green sheet for forming a wavelength converting member may have a thickness of 10 to 2,000 ⁇ m. Specifically, the green sheet for forming a wavelength converting member may have a thickness of 20 to 1,200 ⁇ m.
  • the inorganic phosphor powder since the inorganic phosphor powder neither melts nor reacts at the calcination temperature, it may be used as a material for a confining layer. However, the inorganic phosphor powder must be concentrated at a high density in order to act as a material for a confining layer, and the compacted inorganic phosphor powder may reduce the refractive index and the light transmittance by preventing light from entering the inside of the wavelength converting member. Thus, it is preferable that the green sheet for a confining layer A and the green sheet for a confining layer B does not contain an inorganic phosphor powder.
  • the green sheet for a confining layer A comprises a silica powder only as an inorganic oxide powder.
  • the green sheet for a confining layer A controls the shape of the green sheet for forming a wavelength converting member during the calcination and serves to help the function of the wavelength converting member.
  • a silica powder is excellent in light transmission characteristics, so that it does not cause a decrease in the amount of light. Rather, it remains on the surface of the wavelength converting member upon the calcination and polishing to act as a light diffusing agent, thereby improving the optical characteristics of the wavelength converting member.
  • the silica powder may have an average particle diameter (D 50 ) of 0.1 to 30 ⁇ m. Specifically, the silica powder may have an average particle diameter (D 50 ) of 0.2 to 20 ⁇ m or 0.5 to 10 ⁇ m.
  • the green sheet for a confining layer A may be prepared from a composition for a confining layer A that comprises a silica powder, a binder resin, and a solvent.
  • the composition for a confining layer A may comprise 500 to 1,500 parts by weight of a silica powder per 100 parts by weight of the binder resin.
  • the solvent may be contained in an amount of 30 to 50% by weight based on the total weight of the composition for a confining layer A.
  • the binder resin and the solvent are the same as described above with respect to the green sheet for forming a wavelength converting member.
  • the composition for a confining layer A may further comprise a plasticizer.
  • the kind and content of the plasticizer are the same as described above with respect to the green sheet for forming a wavelength converting member.
  • the composition for a confining layer A may be prepared by mixing a solvent and a binder resin, removing bubbles, and then adding thereto a silica powder, a plasticizer, and the like. Since a solvent having a low boiling point is used in the present invention, the binder resin and the solvent can be mixed at room temperature in the preparation of the composition for a confining layer A.
  • the green sheet for a confining layer A may have a thickness of 5 to 200 ⁇ m. Specifically, the green sheet for a confining layer A may have a thickness of 10 to 200 ⁇ m, to 100 ⁇ m, 10 to 50 ⁇ m, 20 to 100 ⁇ m, 20 to 80 ⁇ m, or 20 to 50 ⁇ m.
  • the green sheet for a confining layer A must be disposed on both sides of the green sheet for forming a wavelength converting member. If the green sheet for a confining layer A is disposed on only one side of the green sheet for forming a wavelength converting member and calcined, the green sheet may be shrunk unevenly, whereby the shape of the wavelength converting member thus prepared may be bent, or cracks may be generated on the wavelength converting member.
  • the green sheet for a confining layer B serves to control the shape of the green sheet for forming a wavelength converting member during the calcination.
  • the green sheet for a confining layer B must be disposed on both sides of the green sheet for a confining layer A, which are not in contact with the green sheet for forming a wavelength converting member. If the green sheet for a confining layer B is disposed on only one side of the green sheet for a confining layer A and calcined, the green sheet may be shrunk unevenly, whereby the shape of the wavelength converting member thus prepared may be bent, or cracks may be generated on the wavelength converting member.
  • the green sheet for a confining layer B may comprise at least one inorganic oxide powder selected from the group consisting of alumina, silica, magnesia, and zirconia. Specifically, the green sheet for a confining layer B may comprise alumina or magnesia.
  • the inorganic oxide powder may have an average particle diameter (D 50 ) of 0.1 to 30 ⁇ m. Specifically, the inorganic oxide powder may have an average particle diameter (D 50 ) of 0.5 to 25 ⁇ m, 0.5 to 20 ⁇ m, or 1 to 15 ⁇ m.
  • the green sheet for a confining layer B may be prepared from a composition for a confining layer B that comprises an inorganic oxide powder, a binder resin, and a solvent.
  • the composition for a confining layer B may comprise 500 to 1,500 parts by weight of an inorganic oxide powder per 100 parts by weight of the binder resin.
  • the solvent may be contained in an amount of 30 to 50% by weight based on the total weight of the composition for a confining layer B.
  • the binder resin and the solvent are the same as described above with respect to the green sheet for forming a wavelength converting member.
  • the composition for a confining layer B may further comprise a plasticizer.
  • the kind and content of the plasticizer are the same as described above with respect to the green sheet for forming a wavelength converting member.
  • the composition for a confining layer B may be prepared by mixing a solvent and a binder resin, removing bubbles, and then adding an inorganic oxide powder, a plasticizer, and the like. Since a solvent having a low boiling point is used in the present invention, the binder resin and the solvent can be mixed at room temperature in the preparation of the composition for a confining layer B.
  • the green sheet for a confining layer B may have a thickness of 5 to 200 ⁇ m. Specifically, the green sheet for a confining layer B may have a thickness of 10 to 200 ⁇ m, 10 to 100 ⁇ m, 10 to 50 ⁇ m, 20 to 100 ⁇ m, 20 to 80 ⁇ m, 20 to 50 ⁇ m, or 30 to 50 ⁇ m.
  • the total number of laminations of the green sheet for a confining layer A and the green sheet for a confining layer B may be 4 to 50. Specifically, the total number of laminations of the green sheet for a confining layer A and the green sheet for a confining layer B may be 4 to 40, 8 to 30, or 10 to 30.
  • the present invention provides a process for preparing a wavelength converting member, which comprises a first step of preparing a green sheet for forming the wavelength converting member, which comprises a glass powder and an inorganic phosphor powder; a second step of disposing a green sheet for a confining layer A, which comprises a silica powder only as an inorganic oxide powder, on both sides of the green sheet for forming the wavelength converting member; a third step of disposing a green sheet for a confining layer B on both sides of the green sheet for the confining layer A, which are not in contact with the green sheet for forming the wavelength converting member, and laminating them to obtain a laminate; a fourth step of calcining the laminate; and a fifth step of removing the calcined confining layer A and confining layer B from the calcined laminate.
  • a green sheet for forming a wavelength converting member which comprises a glass powder and an inorganic phosphor powder, is prepared.
  • the glass powder comprises 0.1 to 15% by mole of P 2 O 5 , 20 to 50% by mole of ZnO, 8 to 40% by mole of SiO 2 , 10 to 30% by mole of B 2 O 3 , 0.1 to 20% by mole of SnO 2 , and 0.1 to 20% by mole of Al 2 O 3 , based on the total number of moles of the glass powder.
  • the glass powder comprises 0.1 to 13% by mole, 0.1 to 10% by mole, or 0.2 to 10% by mole of P 2 O 5 ; 25 to 50% by mole, 25 to 48% by mole, or 28 to 48% by mole of ZnO; 8 to 38% by mole, 8 to 36% by mole, or 8 to 35% by mole of SiO 2 ; 11 to 30% by mole, 11 to 28% by mole, or 11 to 27% by mole of B 2 O 3 ; 0.1 to 20% by mole, 0.1 to 15% by mole, 0.1 to 10% by mole, 0.1 to 8% by mole, or 0.1 to 6% by mole of SnO 2 ; and 0.1 to 20% by mole, 0.1 to 15% by mole, 0.5 to 15% by mole, 1 to 13% by mole, or 1 to 11% by mole of Al 2 O 3 , based on the total number of moles of the glass powder.
  • the glass powder may further comprise at least one oxide selected from the group consisting of BaO, SrO, CaO, Na 2 O, K 2 O, and Li 2 O, and the oxide is contained in an amount of 1 to 60% by mole based on the total number of moles of the glass powder.
  • the glass powder may further comprise at least one alkaline earth metal oxide selected from the group consisting of BaO, SrO, and CaO in an amount of 1 to 30% by mole based on the total number of moles of the glass powder.
  • the glass powder may further comprise at least one alkaline earth metal oxide selected from the group consisting of BaO, SrO, and CaO in an amount of 1 to 20% by mole, 1 to 10% by mole, or 1 to 8% by mole, based on the total number of moles of the glass powder.
  • at least one alkaline earth metal oxide selected from the group consisting of BaO, SrO, and CaO in an amount of 1 to 20% by mole, 1 to 10% by mole, or 1 to 8% by mole, based on the total number of moles of the glass powder.
  • the glass powder may further comprise at least one alkaline metal oxide selected from the group consisting of Na 2 O, K 2 O, and Li 2 O in an amount of 1 to 30% by mole based on the total number of moles of the glass powder. More specifically, the glass powder may further comprise at least one alkaline metal oxide selected from the group consisting of Na 2 O, K 2 O, and Li 2 O in an amount of 1 to 20% by mole, 1 to 18% by mole, or 2 to 17% by mole, based on the total number of moles of the glass powder.
  • the glass powder may comprise 1 to 10% by mole or 1.5 to 8% by mole of Na 2 O; 0 to 10%/o by mole, 0 to 8% by mole, or 0 to 7% by mole of K 2 O; and 0 to 10% by mole, 0 to 8% by mole, or 0 to 7% by mole of Li 2 O, based on the total number moles of the glass powder.
  • the glass powder may have a refractive index of 1.4 to 1.7, a softening point (Ts) of 400 to 700° C., and an average particle diameter (D 50 ) of 0.1 to 20 ⁇ m.
  • the glass powder may have a refractive index of 1.45 to 1.7, 1.5 to 1.66, 1.55 to 1.65, or 1.58 to 1.66, a softening point (Ts) of 400 to 700° C., 500 to 700° C., 550 to 700° C., or 550 to 650° C., and an average particle diameter (D 50 ) of 0.1 to 20 ⁇ m, 1 to 20 ⁇ m, or 1 to 10 ⁇ m.
  • the kind and average particle diameter of the inorganic phosphor powder are the same as described above with respect to the laminate for a wavelength converting member.
  • the green sheet for forming a wavelength converting member may be prepared from a glass composition that comprises a glass powder and an inorganic phosphor powder.
  • the glass composition is the same as described above with respect to the laminate for a wavelength converting member.
  • the green sheet for forming a wavelength converting member may be prepared by casting the glass composition on a substrate.
  • the green sheet for forming a wavelength converting member may be one sheet or may be one obtained by laminating a plurality of green sheets, each of which is prepared by casting, followed by pressing them.
  • the number of laminations of the green sheet is not particularly limited.
  • it may be laminated so that the thickness of the green sheet for forming a wavelength converting member upon pressing is 50 to 1,500 ⁇ m.
  • the pressing may be carried out at a pressure of 1 to 100 MPa. Specifically, the pressing may be carried out at a pressure of 2 to 50 MPa.
  • a green sheet for a confining layer A which comprises a silica powder only as an inorganic oxide powder, is disposed on both sides of the green sheet for forming a wavelength converting member.
  • the silica powder may have an average particle diameter (D 50 ) of 0.1 to 30 ⁇ m. Specifically, the silica powder may have an average particle diameter (D 50 ) of 0.2 to 20 ⁇ m or 0.5 to 10 ⁇ m.
  • the green sheet for a confining layer A may be prepared from a composition for a confining layer A that comprises a silica powder, a binder resin, and a solvent.
  • composition for a confining layer A, the binder resin, and the solvent are the same as described above with respect to the laminate for a wavelength converting member.
  • the green sheet for a confining layer A may have a thickness of 5 to 200 ⁇ m. Specifically, the green sheet for a confining layer A may have a thickness of 10 to 200 ⁇ m, to 100 ⁇ m, 10 to 50 ⁇ m, 20 to 100 ⁇ m, 20 to 80 ⁇ m, or 20 to 50 ⁇ m.
  • a green sheet for a confining layer B is disposed on both sides of the green sheet for a confining layer A, which are not in contact with the green sheet for forming a wavelength converting member, and laminating them to obtain a laminate.
  • the green sheet for a confining layer B may comprise at least one inorganic oxide powder selected from the group consisting of alumina, silica, magnesia, and zirconia. Specifically, the green sheet for a confining layer B may comprise alumina or magnesia.
  • the inorganic oxide powder may have an average particle diameter (DO) of 0.1 to 30 ⁇ m. Specifically, the inorganic oxide powder may have an average particle diameter (D 50 ) of 0.5 to 25 ⁇ m, 0.5 to 20 ⁇ m, or 1 to 15 ⁇ m.
  • the green sheet for a confining layer B may be prepared from a composition for a confining layer B that comprises an inorganic oxide powder, a binder resin, and a solvent.
  • composition for a confining layer B, the binder resin, and the solvent are the same as described above with respect to the laminate for preparing a wavelength converting member.
  • the green sheet for a confining layer B may have a thickness of 5 to 200 ⁇ m. Specifically, the green sheet for a confining layer B may have a thickness of 10 to 200 ⁇ m, 10 to 100 ⁇ m, 10 to 50 ⁇ m, 20 to 100 ⁇ m, 20 to 80 ⁇ m, 20 to 50 ⁇ m, or 30 to 50 ⁇ m.
  • the total number of laminations of the green sheet for a confining layer A and the green sheet for a confining layer B may be 4 to 50. Specifically, the total number of laminations of the green sheet for a confining layer A and the green sheet for a confining layer B may be 4 to 30, 8 to 30, or 10 to 30.
  • the lamination may be carried out for 5 to 90 seconds at a pressure of 12 to 200 MPa and a temperature of 40 to 80° C. Specifically, the lamination may be carried out for 5 to 60 seconds at a pressure of 12 to 180 MPa, 12 to 160 MPa, or 13 to 150 MPa and a temperature of 40 to 70° C. More specifically, the lamination may be carried out using a laminator having an upper part temperature of 60 to 70° C. and a lower part temperature of 40 to 60° C.
  • the laminate is calcined.
  • the calcination may be carried out at 500 to 800° C. for 10 minutes to 72 hours. Specifically, the calcination may be carried out at 500 to 700° C. for 10 minutes to 52 hours.
  • the calcined confining layer A and confining layer B are removed from the calcined laminate.
  • the calcined confining layer A and confining layer B are removed from the calcined laminate by ultrasonic cleaning.
  • the ultrasonic cleaning may be carried out for 5 seconds to 2 hours with an ultrasonic wave of 10,000 to 100,000 Hz.
  • the ultrasonic cleaning may be carried out for 30 seconds to 1 hour with an ultrasonic wave of 30,000 to 50,000 Hz.
  • the wavelength converting member may have a thickness of 100 to 1,000 ⁇ m. Specifically, the wavelength converting member may have a thickness of 100 to 800 ⁇ m, 100 to 500 ⁇ m, or 100 to 300 ⁇ m.
  • the wavelength converting member may have a light transmittance of 70 to 80%. Specifically, the wavelength converting member may have a light transmittance of 72 to 80%, 74 to 78%, or 76 to 78%.
  • the process for preparing a wavelength converting member can efficiently prepare the wavelength converting member using a confining layer comprised of specific components, which can be prepared by the calcination at a temperature of 800° C. or lower, preferably 700° C. or lower and has a high light transmittance, a high refractive index, and a good shape upon the calcination, whereby it can be advantageously used for LEDs.
  • the respective components were mixed to have a composition shown in Table 1 below and melted at 1,200 to 1,400° C. to prepare a glass material.
  • the glass material thus prepared was pulverized to prepare a glass powder having an average particle diameter of 5.9 ⁇ m.
  • the glass powder thus prepared was put into a mold, subjected to compression molding at a pressure of 5 tons for 5 minutes, and then calcined in a furnace at 620° C. for 30 minutes. Thereafter, the mirror surface was abraded to have a surface roughness of 0.2 ⁇ m to prepare a glass plate having a thickness of 200 ⁇ m.
  • Each glass plate was prepared in the same manner as in Preparation Example 1, except that the contents of the respective components were changed to have the composition of Table 1 below.
  • Tg Glass Transition Temperature
  • Ts Softening Temperature
  • the glass transition temperature and the softening temperature were measured using a thermal analyzer (SDT: Q600, TA Instruments, USA) at a temperature elevation rate of 10° C./minute from room temperature to 1,000° C.
  • Tdsp temperature dilatometer softening point
  • the transmittance of light having a reference wavelength of 550 nm was measured using a magnetic spectrophotometer (U-350, Japan) of Hitachi. The light transmittance was 100% when a sample was not present.
  • the refractive index was measured using Professional Gemstone Refractometers (Kruess model ER601 LED, Germany). For the measurement, the specimen was processed to a thickness of 1 mm (1T), and then a certain amount of a refractive solution was applied to the specimen measurement position so as to be in close contact with the measurement portion.
  • the glass plates of Preparation Examples 1 to 10 showed a high transmittance and excellent refractive index characteristics. They had appropriate softening characteristics with a glass transition temperature of 650° C. or less.
  • the light transmittance and the refractive index of a glass matrix affect the optical properties of a wavelength converting member, the characteristics of the wavelength converting members were examined based on these results.
  • Example 1-1 160 g of the binder solution of Example 1-1, 500 g of a silica powder (average particle diameter (D 50 ): 4.9 ⁇ m), and 20 g of a plasticizer were mixed to prepare a composition for confining layer A. Thereafter, a sheet for a confining layer A having a thickness of 30 ⁇ m was prepared from the composition for a confining layer A by the same tape casting method as in Example 1-1.
  • Example 1-1 160 g of the binder solution of Example 1-1, 500 g of an alumina powder (average particle diameter (D 50 ): 2.2 ⁇ m), and 20 g of a plasticizer were mixed to prepare a composition for confining layer B. Thereafter, a sheet for a confining layer B having a thickness of 30 ⁇ m was prepared from the composition for a confining layer B by the same tape casting method as in Example 1-1.
  • the green sheet for a confining layer A of Example 1-2 was disposed on both sides of the green sheet for forming a wavelength converting member of Example 1-1. Thereafter, the green sheet for a confining layer B of Example 1-3 was disposed on both sides of the green sheet for a confining layer A, which were not in contact with the green sheet for forming a wavelength converting member, to prepare a laminate.
  • the laminate was put into a laminator having an upper part temperature of 65° C. and a lower part temperature of 50° C. and pressed for 30 seconds at a pressure of 14 MPa.
  • the pressed laminate was put into a furnace at 600° C., calcined for 0.5 hour, and then subject to ultrasonic cleaning for 10 minutes using an ultrasonic wave of 45,000 Hz to remove the calcined confining layers A and B, thereby obtaining a wavelength converting member having an average thickness of 100 ⁇ m.
  • Each wavelength converting member was prepared in the same manner as in Example 1, except that the kind of the glass powder and the kind of the inorganic oxide contained in the green sheet for a confining layer A and the green sheet for a confining layer B were changed as shown in Table 2 below.
  • the calcination state of the wavelength converting member was evaluated by the naked eyes.
  • the transmittance of light having a reference wavelength of 550 nm was measured using a magnetic spectrophotometer (U-350, Japan) of Hitachi. The light transmittance was 100% when a sample was not present.
  • the chromaticity distribution was measured by placing a wavelength converting member on an excitation light source of 445 nm in an integrating sphere measuring device (LMS-200, J & C Tech.).
  • the wavelength converting members thus prepared had differences in the optical properties due to the differences in transmittance according to the glass compositions.
  • the wavelength converting members of Examples 4 to 6 showed remarkably excellent optical characteristics.
  • the wavelength converting members of Comparative Examples 1 to 4 had a significantly low transmittance and remarkably low optical characteristics as well.

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Abstract

The present invention relates to a laminate for preparing a wavelength converting member and a process for preparing a wavelength converting member. More particularly, the present invention relates to a laminate for preparing a wavelength converting member, which can be calcined at a temperature of 800° C. or lower, preferably 700° C. or lower and has a high light transmittance, a high refractive index, and a good shape upon the calcination, whereby it can be advantageously used for LEDs, and a process for efficiently preparing the wavelength converting member using a confining layer comprised of specific components.

Description

TECHNICAL FIELD
The present invention relates to a laminate for preparing a wavelength converting member and a process for preparing a wavelength converting member. More particularly, the present invention relates to a laminate for preparing a wavelength converting member having a high total light transmittance and excellent optical characteristics, and a process for efficiently preparing the wavelength converting member using a confining layer comprised of specific components.
BACKGROUND ART
Light emitting diodes (LEDs) used for conventional lighting and the like are generally composed of blue LEDs and wavelength converting members that absorb blue light emitted from the blue LEDs and achieve white light through the emission of yellow, green, or red light.
The wavelength converting member may be prepared by preparing a green sheet for forming a wavelength converting member that generally comprises glass, followed by laminating a confining layer for controlling the shape of the green sheet on one side or both sides of the green sheet and calcining the laminate. However, if the confining layer is laminated on only one side of the green sheet and calcined, the green sheet may be shrunk unevenly during the calcination, thereby impairing the shape of the wavelength converting member thus prepared.
As a specific example of the process for preparing a conventional wavelength converting member, Korean Patent No. 10-0930165 discloses a process of disposing a first confining layer that comprises an alumina powder on both sides of a green sheet that comprises a glass component and disposing a second confining layer that comprises a combustible material on each of the exposed sides of the first confining layer, thereby preparing a multilayered ceramic substrate. According to the preparation process of the above patent, however, the green sheet melt, i.e., a glass melt, which has a low viscosity at a high temperature during calcination after the lamination, penetrates between the alumina particles used as a component of the first confining layer to form a thin layer on the interface between the two layers. While the confining layers are removed by polishing and/or etching after the calcination, the layer formed between the green sheet and the confining layer is not completely removed but remains on the surface of the wavelength converting member, thereby reflecting light emitted from a light source. Thus, it has a disadvantage that the amount of light to reach a phosphor is reduced.
DETAILED DESCRIPTION OF THE INVENTION Technical Problem
An object of the present invention is to provide a laminate for preparing a wavelength converting member, which is capable of being calcined at a temperature of 800° C. or lower, preferably 700° C. or lower and having a high light transmittance, a high refractive index, and a good shape upon the calcination, and a process for efficiently preparing the wavelength converting member.
Solution to the Problem
In order to accomplish the above object, the present invention provides a laminate for preparing a wavelength converting member, which comprises a green sheet for forming the wavelength converting member, which comprises a glass matrix and an inorganic phosphor powder dispersed in the glass matrix; a green sheet for a confining layer A, which comprises a silica powder only as an inorganic oxide powder and is disposed on both sides of the green sheet for forming the wavelength converting member; and a green sheet for a confining layer B disposed on both sides of the green sheet for the confining layer A, which are not in contact with the green sheet for forming the wavelength converting member, wherein the glass matrix comprises 0.1 to 15% by mole of P2O5, 20 to 50% by mole of ZnO, 8 to 40% by mole of SiO2, and 10 to 30% by mole of B2O3, based on the total number of moles of the glass powder.
In addition, the present invention provides a process for preparing a wavelength converting member, which comprises a first step of preparing a green sheet for forming the wavelength converting member, which comprises a glass powder and an inorganic phosphor powder; a second step of disposing a green sheet for a confining layer A, which comprises a silica powder only as an inorganic oxide powder, on both sides of the green sheet for forming the wavelength converting member; a third step of disposing a green sheet for a confining layer B on both sides of the green sheet for the confining layer A, which are not in contact with the green sheet for forming the wavelength converting member, and laminating them to obtain a laminate; a fourth step of calcining the laminate; and a fifth step of removing the calcined confining layer A and confining layer B from the calcined laminate.
In addition, the present invention provides a wavelength converting member prepared through the above preparation process.
Advantageous Effects of the Invention
The wavelength converting member according to the present member can be prepared by the calcination at a temperature of 800° C. or lower, preferably 700 IC or lower and has a high light transmittance, a high refractive index, and a good shape upon the calcination. Thus, it can be advantageously used for LEDs.
BEST MODE FOR CARRYING OUT THE INVENTION
The laminate for preparing a wavelength converting member of the present invention comprises a green sheet for forming the wavelength converting member, which comprises a glass matrix and an inorganic phosphor powder dispersed in the glass matrix; a green sheet for a confining layer A, which comprises a silica powder only as an inorganic oxide powder and is disposed on both sides of the green sheet for forming the wavelength converting member; and a green sheet for a confining layer B disposed on both sides of the green sheet for the confining layer A, which are not in contact with the green sheet for forming the wavelength converting member, wherein the glass matrix comprises 0.1 to 15% by mole of P2O5, 20 to 50% by mole of ZnO, 8 to 40% by mole of SiO2, and 10 to 30% by mole of B2O3, based on the total number of moles of the glass powder.
Glass Matrix
The glass matrix comprises 0.1 to 15% by mole of P2O5, 20 to 50% by mole of ZnO, 8 to 40% by mole of SiO2, and 10 to 30% by mole of B2O3, based on the total number of moles of the glass powder. Specifically, the glass matrix comprises 0.1 to 13% by mole, 0.1 to 10% by mole, or 0.2 to 10% by mole of P2O5; 25 to 50% by mole, 25 to 48% by mole, or 28 to 48% by mole of ZnO; 8 to 38% by mole, 8 to 36% by mole, or 8 to 35% by mole of SiO2; and 11 to 30% by mole, 11 to 28% by mole, or 11 to 27% by mole of B2O3, based on the total number of moles of the glass powder.
The glass matrix may further comprise 0.1 to 20% by mole of SnO2 and 0.1 to 20% by mole of Al2O3, based on the total number of moles of the glass powder. Specifically, the glass matrix may further comprise 0.1 to 15% by mole, 0.1 to 10% by mole, 0.1 to 8% by mole, or 0.1 to 6% by mole of SnO2; and 0.1 to 15% by mole, 0.5 to 15% by mole, 1 to 13% by mole, or 1 to 11% by mole of Al2O3, based on the total number of moles of the glass powder.
The glass matrix may further comprise at least one alkaline earth metal oxide selected from the group consisting of BaO, SrO, and CaO in an amount of 1 to 30% by mole based on the total number of moles of the glass powder. Specifically, the glass matrix may further comprise at least one alkaline earth metal oxide selected from the group consisting of BaO, SrO, and CaO in an amount of 1 to 20% by mole, 1 to 10% by mole, or 1 to 8% by mole, based on the total number of moles of the glass powder.
The glass matrix may further comprise at least one alkaline metal oxide selected from the group consisting of Na2O, K2O, and Li2O in an amount of 1 to 30% by mole based on the total number of moles of the glass powder. Specifically, the glass matrix may further comprise at least one alkaline metal oxide selected from the group consisting of Na2O, K2O, and Li2O in an amount of 1 to 20% by mole, 1 to 18% by mole, or 2 to 17% by mole, based on the total number of moles of the glass powder. More specifically, the glass matrix may comprise 1 to 10% by mole or 1.5 to 8% by mole of Na2O; 0 to 10% by mole, 0 to 8% by mole, or 0 to 7% by mole of K2O; and 0 to 10% by mole, 0 to 8% by mole, or 0 to 7% by mole of Li2O, based on the total number moles of the glass powder.
Specifically, the alkaline metal oxide comprises Na2O and K2O; Na2O and Li2O; or Na2O, K2O, and Li2O.
The glass matrix may have a refractive index of 1.4 to 1.7 and may be derived from a glass powder having a softening point (Ts) of 400 to 700° C. and an average particle diameter (D50) of 0.1 to 20 μm. Specifically, the glass matrix may have a refractive index of 1.45 to 1.7, 1.5 to 1.66, 1.55 to 1.65, or 1.58 to 1.66, and may be derived from a glass powder having a softening point (Ts) of 400 to 700° C., 500 to 700° C., 550 to 700° C., or 550 to 650° C., and an average particle diameter (D50) of 0.1 to 20 μm, 1 to 20 μm, or 1 to 10 μm.
Inorganic Phosphor Powder
The inorganic phosphor powder may comprise at least one phosphor powder selected from the group consisting of yttrium-aluminum-garnet (YAG)-based, ruthenium-aluminum-garnet (LuAG)-based, nitride-based, sulfide-based, and silicate-based materials.
The inorganic phosphor powder may have an average particle diameter (D50) of 1 to 50 μm. Specifically, the inorganic phosphor powder may have an average particle diameter (D50) of 1 to 50 μm, 5 to 40 μm, or 10 to 30 μm.
Green Sheet for Forming a Wavelength Converting Member
The green sheet for forming a wavelength converting member comprises a glass matrix and an inorganic phosphor powder dispersed in the glass matrix.
The green sheet for forming a wavelength converting member may be prepared from a glass composition that comprises a glass powder, an inorganic phosphor powder, a binder resin, and a solvent. Specifically, the glass composition may comprise 3 to 160 parts by weight of an inorganic phosphor powder and 120 to 280 parts by weight of a glass powder per 100 parts by weight of a binder resin.
The solvent may be contained in an amount suitable for the characteristics and drying conditions of the composition. Specifically, the solvent may be contained in an amount of 30 to 50% by weight based on the total weight of the glass composition.
The solvent may have a low boiling point for the rapid preparation of the green sheet. Specifically, the solvent may have a boiling point of 30 to 150° C. More specifically, the solvent may have a boiling point of 60 to 130° C.
In addition, the solvent may comprise at least one selected from the group consisting of toluene, ethanol, butanol, acetone, and methanol. Specifically, the solvent may comprise at least one selected from the group consisting of toluene, ethanol, and butanol. More specifically, the solvent may comprise toluene, ethanol, and butanol.
The binder resin may comprise at least one selected from the group consisting of polyvinyl butyral (PVB), polyvinyl alcohol (PVA), and poly(vinyl acetate) (PVAc). Specifically, the binder resin may comprise polyvinyl butyral (PVB) or polyvinyl alcohol (PVA).
The binder resin may have a weight average molecular weight of 1,000 to 70,000 g/mole. Specifically, the binder resin may have a weight average molecular weight of 20,000 to 60,000 g/mole.
The glass composition may further comprise a plasticizer. The plasticizer may comprise at least one selected from the group consisting of DOP (dioctyl phthalate), DOA (dioctyl adipate), and TCP (tricresyl phosphate). Specifically, the plasticizer may comprise DOP (dioctyl phthalate) or DOA (dioctyl adipate).
In addition, the plasticizer may be contained in an amount of 10 to 200 parts by weight per 100 parts by weight of the binder resin. Specifically, the plasticizer may be contained in an amount of 30 to 90 parts by weight per 100 parts by weight of the binder resin.
The glass composition may be prepared by mixing a solvent and a binder resin, removing bubbles, and then adding thereto a glass powder, an inorganic phosphor powder, a plasticizer, and the like. Since a solvent having a low boiling point is used in the present invention, the binder resin and the solvent can be mixed at room temperature in the preparation of the glass composition.
The green sheet for forming a wavelength converting member may comprise 30 to 100% by weight of a glass matrix and 5 to 50% by weight of an inorganic phosphor powder based on the total weight of the green sheet. Specifically, the green sheet for forming a wavelength converting member may comprise 40 to 90% by weight of a glass matrix and 8 to 30% by weight of an inorganic phosphor powder based on the total weight of the green sheet.
The green sheet for forming a wavelength converting member may have a thickness of 10 to 2,000 μm. Specifically, the green sheet for forming a wavelength converting member may have a thickness of 20 to 1,200 μm.
Since the inorganic phosphor powder neither melts nor reacts at the calcination temperature, it may be used as a material for a confining layer. However, the inorganic phosphor powder must be concentrated at a high density in order to act as a material for a confining layer, and the compacted inorganic phosphor powder may reduce the refractive index and the light transmittance by preventing light from entering the inside of the wavelength converting member. Thus, it is preferable that the green sheet for a confining layer A and the green sheet for a confining layer B does not contain an inorganic phosphor powder.
Green Sheet for a Confining Layer A
The green sheet for a confining layer A comprises a silica powder only as an inorganic oxide powder. In addition, the green sheet for a confining layer A controls the shape of the green sheet for forming a wavelength converting member during the calcination and serves to help the function of the wavelength converting member.
Unlike alumina, which reacts with a green sheet melt to form a chemical layer that reflects light to reduce the amount of light that reaches a phosphor, a silica powder is excellent in light transmission characteristics, so that it does not cause a decrease in the amount of light. Rather, it remains on the surface of the wavelength converting member upon the calcination and polishing to act as a light diffusing agent, thereby improving the optical characteristics of the wavelength converting member.
The silica powder may have an average particle diameter (D50) of 0.1 to 30 μm. Specifically, the silica powder may have an average particle diameter (D50) of 0.2 to 20 μm or 0.5 to 10 μm.
The green sheet for a confining layer A may be prepared from a composition for a confining layer A that comprises a silica powder, a binder resin, and a solvent. Specifically, the composition for a confining layer A may comprise 500 to 1,500 parts by weight of a silica powder per 100 parts by weight of the binder resin.
The solvent may be contained in an amount of 30 to 50% by weight based on the total weight of the composition for a confining layer A.
The binder resin and the solvent are the same as described above with respect to the green sheet for forming a wavelength converting member.
The composition for a confining layer A may further comprise a plasticizer. The kind and content of the plasticizer are the same as described above with respect to the green sheet for forming a wavelength converting member.
The composition for a confining layer A may be prepared by mixing a solvent and a binder resin, removing bubbles, and then adding thereto a silica powder, a plasticizer, and the like. Since a solvent having a low boiling point is used in the present invention, the binder resin and the solvent can be mixed at room temperature in the preparation of the composition for a confining layer A.
The green sheet for a confining layer A may have a thickness of 5 to 200 μm. Specifically, the green sheet for a confining layer A may have a thickness of 10 to 200 μm, to 100 μm, 10 to 50 μm, 20 to 100 μm, 20 to 80 μm, or 20 to 50 μm.
The green sheet for a confining layer A must be disposed on both sides of the green sheet for forming a wavelength converting member. If the green sheet for a confining layer A is disposed on only one side of the green sheet for forming a wavelength converting member and calcined, the green sheet may be shrunk unevenly, whereby the shape of the wavelength converting member thus prepared may be bent, or cracks may be generated on the wavelength converting member.
Green Sheet for a Confining Layer B
The green sheet for a confining layer B serves to control the shape of the green sheet for forming a wavelength converting member during the calcination.
The green sheet for a confining layer B must be disposed on both sides of the green sheet for a confining layer A, which are not in contact with the green sheet for forming a wavelength converting member. If the green sheet for a confining layer B is disposed on only one side of the green sheet for a confining layer A and calcined, the green sheet may be shrunk unevenly, whereby the shape of the wavelength converting member thus prepared may be bent, or cracks may be generated on the wavelength converting member.
The green sheet for a confining layer B may comprise at least one inorganic oxide powder selected from the group consisting of alumina, silica, magnesia, and zirconia. Specifically, the green sheet for a confining layer B may comprise alumina or magnesia.
The inorganic oxide powder may have an average particle diameter (D50) of 0.1 to 30 μm. Specifically, the inorganic oxide powder may have an average particle diameter (D50) of 0.5 to 25 μm, 0.5 to 20 μm, or 1 to 15 μm.
The green sheet for a confining layer B may be prepared from a composition for a confining layer B that comprises an inorganic oxide powder, a binder resin, and a solvent. Specifically, the composition for a confining layer B may comprise 500 to 1,500 parts by weight of an inorganic oxide powder per 100 parts by weight of the binder resin.
The solvent may be contained in an amount of 30 to 50% by weight based on the total weight of the composition for a confining layer B.
The binder resin and the solvent are the same as described above with respect to the green sheet for forming a wavelength converting member.
The composition for a confining layer B may further comprise a plasticizer. The kind and content of the plasticizer are the same as described above with respect to the green sheet for forming a wavelength converting member.
The composition for a confining layer B may be prepared by mixing a solvent and a binder resin, removing bubbles, and then adding an inorganic oxide powder, a plasticizer, and the like. Since a solvent having a low boiling point is used in the present invention, the binder resin and the solvent can be mixed at room temperature in the preparation of the composition for a confining layer B.
The green sheet for a confining layer B may have a thickness of 5 to 200 μm. Specifically, the green sheet for a confining layer B may have a thickness of 10 to 200 μm, 10 to 100 μm, 10 to 50 μm, 20 to 100 μm, 20 to 80 μm, 20 to 50 μm, or 30 to 50 μm.
The total number of laminations of the green sheet for a confining layer A and the green sheet for a confining layer B may be 4 to 50. Specifically, the total number of laminations of the green sheet for a confining layer A and the green sheet for a confining layer B may be 4 to 40, 8 to 30, or 10 to 30.
Process for Preparing a Wavelength Converting Member
The present invention provides a process for preparing a wavelength converting member, which comprises a first step of preparing a green sheet for forming the wavelength converting member, which comprises a glass powder and an inorganic phosphor powder; a second step of disposing a green sheet for a confining layer A, which comprises a silica powder only as an inorganic oxide powder, on both sides of the green sheet for forming the wavelength converting member; a third step of disposing a green sheet for a confining layer B on both sides of the green sheet for the confining layer A, which are not in contact with the green sheet for forming the wavelength converting member, and laminating them to obtain a laminate; a fourth step of calcining the laminate; and a fifth step of removing the calcined confining layer A and confining layer B from the calcined laminate.
First Step
In this step, a green sheet for forming a wavelength converting member, which comprises a glass powder and an inorganic phosphor powder, is prepared.
The glass powder comprises 0.1 to 15% by mole of P2O5, 20 to 50% by mole of ZnO, 8 to 40% by mole of SiO2, 10 to 30% by mole of B2O3, 0.1 to 20% by mole of SnO2, and 0.1 to 20% by mole of Al2O3, based on the total number of moles of the glass powder. Specifically, the glass powder comprises 0.1 to 13% by mole, 0.1 to 10% by mole, or 0.2 to 10% by mole of P2O5; 25 to 50% by mole, 25 to 48% by mole, or 28 to 48% by mole of ZnO; 8 to 38% by mole, 8 to 36% by mole, or 8 to 35% by mole of SiO2; 11 to 30% by mole, 11 to 28% by mole, or 11 to 27% by mole of B2O3; 0.1 to 20% by mole, 0.1 to 15% by mole, 0.1 to 10% by mole, 0.1 to 8% by mole, or 0.1 to 6% by mole of SnO2; and 0.1 to 20% by mole, 0.1 to 15% by mole, 0.5 to 15% by mole, 1 to 13% by mole, or 1 to 11% by mole of Al2O3, based on the total number of moles of the glass powder.
The glass powder may further comprise at least one oxide selected from the group consisting of BaO, SrO, CaO, Na2O, K2O, and Li2O, and the oxide is contained in an amount of 1 to 60% by mole based on the total number of moles of the glass powder. Specifically, the glass powder may further comprise at least one alkaline earth metal oxide selected from the group consisting of BaO, SrO, and CaO in an amount of 1 to 30% by mole based on the total number of moles of the glass powder. More specifically, the glass powder may further comprise at least one alkaline earth metal oxide selected from the group consisting of BaO, SrO, and CaO in an amount of 1 to 20% by mole, 1 to 10% by mole, or 1 to 8% by mole, based on the total number of moles of the glass powder.
Specifically, the glass powder may further comprise at least one alkaline metal oxide selected from the group consisting of Na2O, K2O, and Li2O in an amount of 1 to 30% by mole based on the total number of moles of the glass powder. More specifically, the glass powder may further comprise at least one alkaline metal oxide selected from the group consisting of Na2O, K2O, and Li2O in an amount of 1 to 20% by mole, 1 to 18% by mole, or 2 to 17% by mole, based on the total number of moles of the glass powder. Even more specifically, the glass powder may comprise 1 to 10% by mole or 1.5 to 8% by mole of Na2O; 0 to 10%/o by mole, 0 to 8% by mole, or 0 to 7% by mole of K2O; and 0 to 10% by mole, 0 to 8% by mole, or 0 to 7% by mole of Li2O, based on the total number moles of the glass powder.
The glass powder may have a refractive index of 1.4 to 1.7, a softening point (Ts) of 400 to 700° C., and an average particle diameter (D50) of 0.1 to 20 μm. Specifically, the glass powder may have a refractive index of 1.45 to 1.7, 1.5 to 1.66, 1.55 to 1.65, or 1.58 to 1.66, a softening point (Ts) of 400 to 700° C., 500 to 700° C., 550 to 700° C., or 550 to 650° C., and an average particle diameter (D50) of 0.1 to 20 μm, 1 to 20 μm, or 1 to 10 μm.
The kind and average particle diameter of the inorganic phosphor powder are the same as described above with respect to the laminate for a wavelength converting member.
The green sheet for forming a wavelength converting member may be prepared from a glass composition that comprises a glass powder and an inorganic phosphor powder. The glass composition is the same as described above with respect to the laminate for a wavelength converting member.
The green sheet for forming a wavelength converting member may be prepared by casting the glass composition on a substrate. Specifically, the green sheet for forming a wavelength converting member may be one sheet or may be one obtained by laminating a plurality of green sheets, each of which is prepared by casting, followed by pressing them. In such event, the number of laminations of the green sheet is not particularly limited. For example, it may be laminated so that the thickness of the green sheet for forming a wavelength converting member upon pressing is 50 to 1,500 μm.
The pressing may be carried out at a pressure of 1 to 100 MPa. Specifically, the pressing may be carried out at a pressure of 2 to 50 MPa.
Second Step
In this step, a green sheet for a confining layer A, which comprises a silica powder only as an inorganic oxide powder, is disposed on both sides of the green sheet for forming a wavelength converting member.
The silica powder may have an average particle diameter (D50) of 0.1 to 30 μm. Specifically, the silica powder may have an average particle diameter (D50) of 0.2 to 20 μm or 0.5 to 10 μm.
The green sheet for a confining layer A may be prepared from a composition for a confining layer A that comprises a silica powder, a binder resin, and a solvent.
The composition for a confining layer A, the binder resin, and the solvent are the same as described above with respect to the laminate for a wavelength converting member.
The green sheet for a confining layer A may have a thickness of 5 to 200 μm. Specifically, the green sheet for a confining layer A may have a thickness of 10 to 200 μm, to 100 μm, 10 to 50 μm, 20 to 100 μm, 20 to 80 μm, or 20 to 50 μm.
Third Step
In this step, a green sheet for a confining layer B is disposed on both sides of the green sheet for a confining layer A, which are not in contact with the green sheet for forming a wavelength converting member, and laminating them to obtain a laminate.
The green sheet for a confining layer B may comprise at least one inorganic oxide powder selected from the group consisting of alumina, silica, magnesia, and zirconia. Specifically, the green sheet for a confining layer B may comprise alumina or magnesia. The inorganic oxide powder may have an average particle diameter (DO) of 0.1 to 30 μm. Specifically, the inorganic oxide powder may have an average particle diameter (D50) of 0.5 to 25 μm, 0.5 to 20 μm, or 1 to 15 μm.
The green sheet for a confining layer B may be prepared from a composition for a confining layer B that comprises an inorganic oxide powder, a binder resin, and a solvent.
The composition for a confining layer B, the binder resin, and the solvent are the same as described above with respect to the laminate for preparing a wavelength converting member.
The green sheet for a confining layer B may have a thickness of 5 to 200 μm. Specifically, the green sheet for a confining layer B may have a thickness of 10 to 200 μm, 10 to 100 μm, 10 to 50 μm, 20 to 100 μm, 20 to 80 μm, 20 to 50 μm, or 30 to 50 μm.
The total number of laminations of the green sheet for a confining layer A and the green sheet for a confining layer B may be 4 to 50. Specifically, the total number of laminations of the green sheet for a confining layer A and the green sheet for a confining layer B may be 4 to 30, 8 to 30, or 10 to 30.
The lamination may be carried out for 5 to 90 seconds at a pressure of 12 to 200 MPa and a temperature of 40 to 80° C. Specifically, the lamination may be carried out for 5 to 60 seconds at a pressure of 12 to 180 MPa, 12 to 160 MPa, or 13 to 150 MPa and a temperature of 40 to 70° C. More specifically, the lamination may be carried out using a laminator having an upper part temperature of 60 to 70° C. and a lower part temperature of 40 to 60° C.
Fourth Step
In this step, the laminate is calcined.
The calcination may be carried out at 500 to 800° C. for 10 minutes to 72 hours. Specifically, the calcination may be carried out at 500 to 700° C. for 10 minutes to 52 hours.
Fifth Step
In this step, the calcined confining layer A and confining layer B are removed from the calcined laminate. Specifically, in this step, the calcined confining layer A and confining layer B are removed from the calcined laminate by ultrasonic cleaning. In such event, the ultrasonic cleaning may be carried out for 5 seconds to 2 hours with an ultrasonic wave of 10,000 to 100,000 Hz. Specifically, the ultrasonic cleaning may be carried out for 30 seconds to 1 hour with an ultrasonic wave of 30,000 to 50,000 Hz.
The wavelength converting member may have a thickness of 100 to 1,000 μm. Specifically, the wavelength converting member may have a thickness of 100 to 800 μm, 100 to 500 μm, or 100 to 300 μm.
The wavelength converting member may have a light transmittance of 70 to 80%. Specifically, the wavelength converting member may have a light transmittance of 72 to 80%, 74 to 78%, or 76 to 78%.
As described above, the process for preparing a wavelength converting member can efficiently prepare the wavelength converting member using a confining layer comprised of specific components, which can be prepared by the calcination at a temperature of 800° C. or lower, preferably 700° C. or lower and has a high light transmittance, a high refractive index, and a good shape upon the calcination, whereby it can be advantageously used for LEDs.
EMBODIMENTS FOR CARRYING OUT THE INVENTION
Hereinafter, the present invention will be described in more detail with reference to the following examples. However, these examples are provided to illustrate the present invention, and the scope of the present invention is not limited thereto only.
EXAMPLE Preparation Example 1: Preparation of a Glass Plate
The respective components were mixed to have a composition shown in Table 1 below and melted at 1,200 to 1,400° C. to prepare a glass material. The glass material thus prepared was pulverized to prepare a glass powder having an average particle diameter of 5.9 μm. The glass powder thus prepared was put into a mold, subjected to compression molding at a pressure of 5 tons for 5 minutes, and then calcined in a furnace at 620° C. for 30 minutes. Thereafter, the mirror surface was abraded to have a surface roughness of 0.2 μm to prepare a glass plate having a thickness of 200 μm.
Preparation Examples 2 to 12
Each glass plate was prepared in the same manner as in Preparation Example 1, except that the contents of the respective components were changed to have the composition of Table 1 below.
Test Example 1
The physical properties of the glass plates of Preparation Examples 1 to 12 were evaluated in the following manner, and the results are shown in Table 1 below.
(1) Glass Transition Temperature (Tg) and Softening Temperature (Ts)
The glass transition temperature and the softening temperature were measured using a thermal analyzer (SDT: Q600, TA Instruments, USA) at a temperature elevation rate of 10° C./minute from room temperature to 1,000° C.
In such event, Tdsp (temperature dilatometer softening point) refers to the temperature of a dilatometer softening point.
(2) Light Transmittance (%)
The transmittance of light having a reference wavelength of 550 nm was measured using a magnetic spectrophotometer (U-350, Japan) of Hitachi. The light transmittance was 100% when a sample was not present.
(3) Refractive Index
The refractive index was measured using Professional Gemstone Refractometers (Kruess model ER601 LED, Germany). For the measurement, the specimen was processed to a thickness of 1 mm (1T), and then a certain amount of a refractive solution was applied to the specimen measurement position so as to be in close contact with the measurement portion.
TABLE 1
Prep. Prep. Prep. Prep. Prep. Prep. Prep. Prep. Prep. Prep. Prep. Prep.
(No. of moles) Ex. 1 Ex. 2 Ex. 3 Ex. 4 Ex. 5 Ex. 6 Ex. 7 Ex. 8 Ex. 9 Ex. 10 Ex. 11 Ex. 12
Comp. P2O5 5.2 3.2 5.8 2.2 0.3 5.3 9.5 5.0 5.2 3.7 — 0.8
ZnO 33.5 45.7 36.6 36.0 29.0 34.0 38.0 34.2 30.6 35.2 39.9 46.4
SiO2 17.8 10.0 20.8 21.6 33.0 18.9 14.3 20.2 20.1 25.3 20.0 7.6
B2O3 18.6 26.8 12.5 21.6 21.0 18.9 19.0 15.1 12.5 15.6 19.0 26.2
Al2O3 3.7 2.0 4.2 7.2 1.1 3.8 2.9 2.0 10.5 1.4 — 0.3
SnO2 5.2 0.1 1.7 0.7 0.2 2.3 0.5 0.1 1.7 1.4 — —
BaO — 2.8 4.2 — 2.4 3.8 4.8 1.1 4.2 3.7 4.8 4.2
SrO — — — — — — — 3.0 — — — —
CaO 3.7 3.0 — 7.2 — — 1.9 3.0 — — — —
Li2O 2.6 — 3.3 — 6.6 3.0 1.4 4.0 4.0 2.0 3.8 3.3
Na2O 5.7 2.8 6.3 1.8 6.4 5.8 5.3 7.7 5.3 5.5 7.2 6.4
K2O 4.0 3.5 4.7 1.8 — 4.2 2.5 4.6 5.0 6.3 5.3 4.7
Avg. particle 5.71 5.82 5.59 5.79 5.50 5.61 5.34 5.54 5.80 5.60 5.73 5.41
diameter
(D50) (μm)
TC* Tg 464 512 453 471 456 455 437 450 479 478 463 430
(° C.) Tdsp 514 524 503 521 495 505 481 499 522 504 516 487
Ts 596 611 586 612 632 589 579 582 608 599 594 559
Light 69.3 58.2 72.2 69.2 38.8 76.9 62.1 69.8 68.9 72.1 34.6 45.3
transmittance
(%)
Refractive 1.65 1.59 1.59 1.59 1.59 1.61 1.59 1.59 1.6 1.6 1.59 1.64
index
*TC: thermal characteristics
As shown in Table 1, the glass plates of Preparation Examples 1 to 10 showed a high transmittance and excellent refractive index characteristics. They had appropriate softening characteristics with a glass transition temperature of 650° C. or less. In addition, since the light transmittance and the refractive index of a glass matrix affect the optical properties of a wavelength converting member, the characteristics of the wavelength converting members were examined based on these results.
Example 1: Preparation of a Wavelength Converting Member
1-1: Preparation of a Green Sheet for Forming a Wavelength Converting Member
27 g of polyvinyl butyral (PVB, weight average molecular weight: 50,000 g/mole) was added to 81 g of a solvent (a mixture of toluene, ethanol, and butanol at a volume ratio of 3:1:1) and dissolved at room temperature for 1 hour to prepare a binder solution.
11 parts by weight of a YAG-based phosphor powder (average particle diameter (D50): 25 μm, manufacturer: Daejoo Electronic Materials, product name: DLP-Y62-25) and 89 parts by weight of the glass powder of Preparation Example 5 were mixed, to which 89 parts by weight of the binder solution and 11 parts by weight of a plasticizer were added to prepare a glass composition. The glass composition was applied to a PET film by a tape casting method and molded into a sheet to obtain a green sheet having a thickness of 50 μm. 21 of the above green sheet were laminated and pressed at a pressure of 14 MPa to obtain a green sheet for forming a wavelength converting member.
1-2: Preparation of a Green Sheet for a Confining Layer A
160 g of the binder solution of Example 1-1, 500 g of a silica powder (average particle diameter (D50): 4.9 μm), and 20 g of a plasticizer were mixed to prepare a composition for confining layer A. Thereafter, a sheet for a confining layer A having a thickness of 30 μm was prepared from the composition for a confining layer A by the same tape casting method as in Example 1-1.
1-3: Preparation of a Green Sheet for a Confining Layer B
160 g of the binder solution of Example 1-1, 500 g of an alumina powder (average particle diameter (D50): 2.2 μm), and 20 g of a plasticizer were mixed to prepare a composition for confining layer B. Thereafter, a sheet for a confining layer B having a thickness of 30 μm was prepared from the composition for a confining layer B by the same tape casting method as in Example 1-1.
1-4: Preparation of a Wavelength Converting Member
The green sheet for a confining layer A of Example 1-2 was disposed on both sides of the green sheet for forming a wavelength converting member of Example 1-1. Thereafter, the green sheet for a confining layer B of Example 1-3 was disposed on both sides of the green sheet for a confining layer A, which were not in contact with the green sheet for forming a wavelength converting member, to prepare a laminate. The laminate was put into a laminator having an upper part temperature of 65° C. and a lower part temperature of 50° C. and pressed for 30 seconds at a pressure of 14 MPa. Thereafter, the pressed laminate was put into a furnace at 600° C., calcined for 0.5 hour, and then subject to ultrasonic cleaning for 10 minutes using an ultrasonic wave of 45,000 Hz to remove the calcined confining layers A and B, thereby obtaining a wavelength converting member having an average thickness of 100 μm.
Examples 2 to 6 and Comparative Examples 1 to 4
Each wavelength converting member was prepared in the same manner as in Example 1, except that the kind of the glass powder and the kind of the inorganic oxide contained in the green sheet for a confining layer A and the green sheet for a confining layer B were changed as shown in Table 2 below.
Test Example 2
The properties of the wavelength converting members of Examples 1 to 6 and Comparative Examples 1 to 4 were measured in the following manners, and the results are shown in Table 2 below.
(1) State of the Calcined Body
The calcination state of the wavelength converting member was evaluated by the naked eyes.
(2) Light Transmittance (%)
The transmittance of light having a reference wavelength of 550 nm was measured using a magnetic spectrophotometer (U-350, Japan) of Hitachi. The light transmittance was 100% when a sample was not present.
(3) Chromaticity Distribution (Cx, Cy, Luminous Flux (Φv, Lumen (lm)), and Converted Luminous Flux (%))
The chromaticity distribution was measured by placing a wavelength converting member on an excitation light source of 445 nm in an integrating sphere measuring device (LMS-200, J & C Tech.).
TABLE 2
Example Comparative Example
1 2 3 4 5 6 1 2 3 4
Glass powder Prep. Prep. Prep. Prep. Prep. Prep. Prep. Prep. Prep. Prep.
Ex. 5 Ex. 5 Ex. 6 Ex. 6 Ex. 10 Ex. 10 Ex. 11 Ex. 11 Ex. 12 Ex. 12
Green Sheet for SiO2 SiO2 SiO2 SiO2 SiO2 SiO2 Al2O3 SiO2 Al2O3 —
a Confining
Layer A
Green Sheet for Al2O3 MgO Al2O3 MgO Al2O3 MgO Al2O3 — — —
a Confining
Layer B
State of Good Good Good Good Good Good Good Bent Good Cracked
calcined body
Light 74.2 74.2 76.9 76.9 72.1 72.1 34.6 34.6 45.3 45.3
transmittance
(%)
Cx 0.292 0.307 0.292 0.301 0.297 0.302 0.355 — 0.338 —
Cy 0.271 0.302 0.272 0.289 0.277 0.293 0.391 — 0.367 —
Luminous flux 80.0 84.1 80.1 82.5 80.7 84.1 80.2 — 81.4 —
(lm)
Converted 98.9 98.1 98.9 100.2 100.0 102.2 79.6 — 79.4 —
luminous flux
(%)
As shown in Table 2, the wavelength converting members thus prepared had differences in the optical properties due to the differences in transmittance according to the glass compositions. In particular, the wavelength converting members of Examples 4 to 6 showed remarkably excellent optical characteristics.
In contrast, the wavelength converting members of Comparative Examples 1 to 4 had a significantly low transmittance and remarkably low optical characteristics as well.

Claims (18)

The invention claimed is:
1. A laminate for preparing a wavelength converting member, which comprises
a first green sheet for forming the wavelength converting member, said first green sheet comprising a glass matrix formed of glass powder and an inorganic phosphor powder dispersed in the glass matrix;
a second green sheet for a confining layer A, which comprises a silica powder only as an inorganic oxide powder and is disposed on both sides of the first green sheet for forming the wavelength converting member; and
a third green sheet for a confining layer B disposed on both sides of the second green sheet for the confining layer A, said both sides of the second green sheet being not in contact with the first green sheet for forming the wavelength converting member,
wherein the glass matrix comprises 0.1 to 15% by mole of P2O5, 20 to 50% by mole of ZnO, 8 to 40% by mole of SiO2, 10 to 30% by mole of B2O3, 0.1 to 20% by mole of SnO2, 0.1 to 20% by mole of Al2O3, and 1 to 30% by mole of K2O, each based on the total number of moles of the glass powder, and
wherein the glass matrix further comprises at least one alkaline earth metal oxide selected from the group consisting of BaO, SrO, and CaO in an amount of 1 to 30% by mole based on the total number of moles of the glass powder;
wherein the third green sheet for the confining layer B comprises at least one inorganic oxide powder selected from the group consisting of alumina, silica, magnesia, and zirconia,
wherein a total number of laminations of the second green sheet for a confining layer A and the third green sheet for a confining layer B is 4 to 50, and
wherein the glass matrix has a refractive index of 1.58 to 1.66 and is derived from the glass powder having a softening point (Ts) of 550 to 650° C. and an average particle diameter (D50) of 1 to 10 μm.
2. The laminate for preparing a wavelength converting member of claim 1, wherein the glass matrix further comprises an alkaline metal oxide selected from the group consisting of Na2O, Li2O, and a mixture thereof, in an amount of 1 to 30% by mole based on the total number of moles of the glass powder.
3. The laminate for preparing a wavelength converting member of claim 1, wherein the inorganic phosphor powder comprises at least one phosphor powder selected from the group consisting of yttrium-aluminum-garnet (YAG)-based, ruthenium-aluminum-garnet (LuAG)-based, nitride-based, sulfide-based, and silicate-based materials.
4. The laminate for preparing a wavelength converting member of claim 1, wherein the inorganic phosphor powder has an average particle diameter (D50) of 1 to 50 μm.
5. The laminate for preparing a wavelength converting member of claim 1, wherein the silica powder of the second green sheet for the confining layer A has an average particle diameter (D50) of 0.1 to 30 μm, and the second green sheet for the confining layer A has a thickness of 5 to 200 μm.
6. The laminate for preparing a wavelength converting member of claim 1, wherein the third green sheet for the confining layer B comprises at least one inorganic oxide powder selected from the group consisting of alumina, silica, magnesia, and zirconia,
the inorganic oxide powder has an average particle diameter (D50) of 0.1 to 30 μm, and
the third green sheet for a confining layer B has a thickness of 5 to 200 μm.
7. A process for preparing a wavelength converting member, which comprises a first step of preparing a first green sheet for forming the wavelength converting member, said green sheet comprising a glass matrix, formed from a glass powder, and an inorganic phosphor powder;
a second step of disposing a second green sheet for a confining layer A, which comprises a silica powder only as an inorganic oxide powder, on both sides of the first green sheet for forming the wavelength converting member;
a third step of disposing a third green sheet for a confining layer B on both sides of the second green sheet for the confining layer A, said both sides of the second green sheet being not in contact with the first green sheet for forming the wavelength converting member, and laminating them to obtain a laminate;
a fourth step of calcining the laminate; and
a fifth step of removing the calcined confining layer A and confining layer B from the calcined laminate,
wherein the glass matrix comprises 0.1 to 15% by mole of P2O5, 20 to 50% by mole of ZnO, 8 to 40% by mole of SiO2, 10 to 30% by mole of B2O3, at least one alkaline earth metal oxide selected from the group consisting of BaO, SrO, and CaO in an amount of 1 to 30% by mole, 0.1 to 20% by mole of SnO2, 0.1 to 20% by mole of Al2O3, and 1 to 30% by mole of K2O, each based on the total number of moles of the glass powder,
wherein the third green sheet for the confining layer B comprises at least one inorganic oxide powder selected from the group consisting of alumina, silica, magnesia, and zirconia,
wherein a total number of laminations of the second green sheet for a confining layer A and the third green sheet for a confining layer B is 4 to 50, and
wherein the glass matrix has a refractive index of 1.58 to 1.66 and is derived from the glass powder having a softening point (Ts) of 550 to 650° C. and an average particle diameter (D50) of 1 to 10 μm.
8. The process for preparing a wavelength converting member of claim 7, wherein the glass powder further comprises an alkaline metal oxide selected from the group consisting of Na2O, Li2O and a mixture thereof in an amount of 1 to 30% by mole based on the total number of moles of the glass powder.
9. The process for preparing a wavelength converting member of claim 7, wherein the inorganic phosphor powder comprises at least one phosphor powder selected from the group consisting of yttrium-aluminum-garnet (YAG)-based, ruthenium-aluminum-garnet (LuAG)-based, nitride-based, sulfide-based, and silicate-based materials.
10. The process for preparing a wavelength converting member of claim 7, wherein the inorganic phosphor powder has an average particle diameter (D50) of 1 to 50 μm.
11. The process for preparing a wavelength converting member of claim 7, wherein the silica powder of the green sheet for the confining layer A has an average particle diameter (D50) of 0.1 to 30 μm, and the green sheet for the confining layer A has a thickness of 5 to 200 μm.
12. The process for preparing a wavelength converting member of claim 7, wherein the third green sheet for the confining layer B comprises at least one inorganic oxide powder selected from the group consisting of alumina, silica, magnesia, and zirconia,
the inorganic oxide powder has an average particle diameter (D50) of 0.1 to 30 μm, and
the green sheet for a confining layer B has a thickness of 5 to 200 μm.
13. The process for preparing a wavelength converting member of claim 7, wherein the lamination in the third step is carried out for 5 to 90 seconds at a pressure of 12 to 200 MPa and a temperature of 40 to 80° C.
14. The process for preparing a wavelength converting member of claim 7, wherein the calcination in the fourth step is carried out at 500 to 800° C. for 10 minutes to 72 hours.
15. The process for preparing a laminate for a wavelength converting member of claim 7, wherein the fifth step is carried out using ultrasonic cleaning.
16. A wavelength converting member prepared through the preparation process of claim 7.
17. The wavelength converting member of claim 16, which has a thickness of 100 to 1,000 μm.
18. The wavelength converting member of claim 16, which has a light transmittance of 70 to 80%.
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